CN104697827A - Preparation and thermal analysis method of alloy sample containing high-volatility elements with high reaction activity - Google Patents
Preparation and thermal analysis method of alloy sample containing high-volatility elements with high reaction activity Download PDFInfo
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- 239000000956 alloy Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000002076 thermal analysis method Methods 0.000 title abstract description 21
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims abstract description 71
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 69
- 239000000843 powder Substances 0.000 claims abstract description 37
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 16
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 15
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 15
- 239000011777 magnesium Substances 0.000 claims abstract description 15
- 239000010453 quartz Substances 0.000 claims abstract description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 15
- 239000011701 zinc Substances 0.000 claims abstract description 15
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 238000000137 annealing Methods 0.000 claims abstract description 8
- 238000005245 sintering Methods 0.000 claims abstract description 7
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 7
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 6
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims abstract description 6
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000010791 quenching Methods 0.000 claims abstract description 6
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 6
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000005464 sample preparation method Methods 0.000 claims abstract 4
- 239000001301 oxygen Substances 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 229910000861 Mg alloy Inorganic materials 0.000 claims description 5
- 238000004458 analytical method Methods 0.000 claims description 5
- 229910000838 Al alloy Inorganic materials 0.000 claims description 4
- 229910000914 Mn alloy Inorganic materials 0.000 claims description 4
- 229910000583 Nd alloy Inorganic materials 0.000 claims description 4
- 229910001278 Sr alloy Inorganic materials 0.000 claims description 4
- 229910001297 Zn alloy Inorganic materials 0.000 claims description 4
- 238000004455 differential thermal analysis Methods 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 3
- 238000000113 differential scanning calorimetry Methods 0.000 claims description 3
- 239000003708 ampul Substances 0.000 claims 3
- 239000004411 aluminium Substances 0.000 claims 2
- 238000007493 shaping process Methods 0.000 claims 2
- 229910052751 metal Inorganic materials 0.000 abstract description 12
- 239000002184 metal Substances 0.000 abstract description 12
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- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 2
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- 229910000946 Y alloy Inorganic materials 0.000 description 2
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- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了一种含高挥发性、高反应活性元素合金样品制备及热分析方法。包括：(1)在手套箱中，称取含高挥发性、高反应活性元素的合金粉末，混合均匀并压制成型；(2)将成型的试样封装入钽管中，再将钽管从手套箱中取出，封入真空石英管中，随后放入热处理炉中进行烧结及退火处理；(3)将石英管从热处理炉中取出迅速淬火并将钽管取出，然后在手套箱中将样品从钽管中取出。本发明的方法可广泛用于镁（铝、锌等）合金、稀土（锰、锶、钇、钕等）合金等含高活性和高挥发性元素的合金的制备及其热分析。通过同标准纯金属物质的熔点对比表明采用本发明的热分析方法测定的相变温度精度可以达到± 1°C。The invention discloses a sample preparation and thermal analysis method of an alloy containing highly volatile and highly reactive elements. Including: (1) In the glove box, weigh the alloy powder containing highly volatile and highly reactive elements, mix it evenly and press it into shape; (2) Pack the formed sample into a tantalum tube, and then put the tantalum tube from Take it out from the glove box, seal it in a vacuum quartz tube, and then put it into a heat treatment furnace for sintering and annealing treatment; (3) Take out the quartz tube from the heat treatment furnace and quickly quench it and take out the tantalum tube, and then take the sample out of the glove box out of the tantalum tube. The method of the invention can be widely used in the preparation and thermal analysis of magnesium (aluminum, zinc, etc.) alloys, rare earth (manganese, strontium, yttrium, neodymium, etc.) alloys containing highly active and highly volatile elements. The comparison of the melting point with the standard pure metal substance shows that the accuracy of the phase transition temperature measured by the thermal analysis method of the present invention can reach ± 1°C.
Description
技术领域 technical field
本发明涉及一种含高挥发性、高反应活性元素合金样品制备及热分析方法。 The invention relates to a method for preparing and thermally analyzing an alloy sample containing highly volatile and highly reactive elements.
背景技术 Background technique
镁、铝、锌等合金作为减重的金属结构材料，具有比强度和比刚度高、导热导电性能好、易于加工和容易回收等特点，在交通运输、电子通信、航空航天等领域得到了广泛的应用。热分析能够提供材料的相变温度，对研究材料的凝固以及固态相变等材料制备过程具有重要的意义。镁、铝、锌等元素的低沸点给研究和应用带来极大的挑战。目前，传统的方法制备合金需要几十克甚至几千克的纯元素原料。开放式的熔炼方法极大地浪费了金属原料，并且挥发的金属蒸汽会污染环境，部分金属蒸汽还有剧毒。此外，开放式的熔炼经常会导致液态金属飞溅，引发安全事故。不含高挥发性、高反应活性元素的材料，其热分析是在非保护气氛中制备样品并在敞开的坩埚中进行的。对于含高挥发、高反应活性元素的镁合金：一方面由于元素的高反应活性，在非保护气氛中制备的样品容易与水、氧发生反应；另一方面由于镁的高挥发性，在热分析过程中随着温度的升高，金属的蒸汽压持续升高。在开放式坩埚中，挥发出的金属蒸汽不断被排出，从而导致了试样的严重挥发，并损坏热分析仪。这两个因素共同作用，导致常规的热分析方法不能用于含高挥发、高反应活性元素的镁、铝、锌等合金的相变温度的测定，从而导致现有镁、铝、锌等合金相图、相变数据非常稀缺。 Magnesium, aluminum, zinc and other alloys, as weight-reducing metal structural materials, have the characteristics of high specific strength and specific stiffness, good thermal and electrical conductivity, easy processing and easy recycling, and have been widely used in transportation, electronic communication, aerospace and other fields. Applications. Thermal analysis can provide the phase transition temperature of materials, which is of great significance to the study of solidification and solid phase transition of materials and other material preparation processes. The low boiling points of magnesium, aluminum, zinc and other elements bring great challenges to research and application. At present, the traditional method of preparing alloys requires dozens of grams or even several kilograms of pure elemental raw materials. The open smelting method greatly wastes metal raw materials, and the volatilized metal vapor will pollute the environment, and some metal vapors are also highly toxic. In addition, open smelting often causes liquid metal to splash, causing safety accidents. Thermal analysis of materials that do not contain highly volatile, highly reactive elements is performed with samples prepared in a non-protective atmosphere and performed in open crucibles. For magnesium alloys containing highly volatile and highly reactive elements: on the one hand, due to the high reactivity of the elements, the samples prepared in a non-protective atmosphere are easy to react with water and oxygen; During the analysis process, as the temperature increases, the vapor pressure of the metal continues to increase. In the open crucible, the volatilized metal vapor is continuously exhausted, resulting in severe volatilization of the sample and damage to the thermal analyzer. These two factors work together, so that the conventional thermal analysis method cannot be used for the determination of the phase transition temperature of magnesium, aluminum, zinc and other alloys containing highly volatile and highly reactive elements, resulting in the existing magnesium, aluminum, zinc and other alloys Phase diagrams and phase transition data are very scarce.
发明内容 Contents of the invention
本发明的目的是提供一种含高挥发性、高反应活性元素合金制备及热分析方法。 The purpose of the present invention is to provide a method for preparing and thermally analyzing an alloy containing highly volatile and highly reactive elements.
为了达到上述目的，本发明的含高挥发性、高反应活性元素合金样品制备方法，包括以下步骤： In order to achieve the above object, the method for preparing an alloy sample containing highly volatile and highly reactive elements of the present invention comprises the following steps:
(1) 在手套箱中，称取含高挥发性、高反应活性元素的合金粉末，混合均匀并压制成型； (1) In the glove box, weigh the alloy powder containing highly volatile and highly reactive elements, mix them evenly and press them into shape;
(2) 将成型的试样封装入钽管中，再将钽管从手套箱中取出，封入真空石英管中，随后放入热处理炉中进行烧结及退火处理； (2) Pack the formed sample into a tantalum tube, then take the tantalum tube out of the glove box, seal it in a vacuum quartz tube, and then put it into a heat treatment furnace for sintering and annealing;
(3) 将石英管从热处理炉中取出迅速淬火并将钽管取出，然后在手套箱中将样品从钽管中取出。 (3) Take the quartz tube out of the heat treatment furnace and quickly quench it and take out the tantalum tube, and then take the sample out of the tantalum tube in the glove box.
优选地，所述的合金粉末为镁合金粉末或者铝合金粉末或者锌合金粉末或者锰合金粉末或者锶合金粉末或者钇合金粉末或者钕合金粉末，其中高挥发性、高反应活性元素镁、铝、锌、锰、锶、钇、钕的含量分别为99.0wt%～99.99wt% 。 Preferably, the alloy powder is magnesium alloy powder or aluminum alloy powder or zinc alloy powder or manganese alloy powder or strontium alloy powder or yttrium alloy powder or neodymium alloy powder, wherein the highly volatile and highly reactive elements magnesium, aluminum, The contents of zinc, manganese, strontium, yttrium and neodymium are respectively 99.0wt% to 99.99wt%.
作为改进，在合金样品制备过程中，保持样品水氧含量为0.4～1.0ppm。 As an improvement, during the preparation of the alloy sample, the water and oxygen content of the sample is kept at 0.4-1.0 ppm.
本发明的含高挥发性、高反应活性元素合金样品的热分析方法，包括以下步骤： The thermal analysis method of the alloy sample containing highly volatile and highly reactive elements of the present invention comprises the following steps:
(1) 在手套箱中，称取含高挥发性、高反应活性元素的合金粉末，混合均匀并压制成型； (1) In the glove box, weigh the alloy powder containing highly volatile and highly reactive elements, mix them evenly and press them into shape;
(2) 将成型的试样封装入钽管中，再将钽管从手套箱中取出，封入真空石英管中，随后放入热处理炉中进行烧结及退火处理； (2) Pack the formed sample into a tantalum tube, then take the tantalum tube out of the glove box, seal it in a vacuum quartz tube, and then put it into a heat treatment furnace for sintering and annealing;
(3) 将石英管从热处理炉中取出迅速淬火并将钽管取出，然后在手套箱中将样品从钽管中取出； (3) Take the quartz tube out of the heat treatment furnace and quickly quench it and take out the tantalum tube, and then take the sample out of the tantalum tube in the glove box;
(4)切取一块重25～60mg的样品作为差示扫描量热分析的试样，用钽片压制出钽盖，将钽盖底部插入长度约10～20mm钽管的一端，并保持钽盖的上部和钽管的底部边缘齐平，再在手套箱中将钽盖和钽管焊接密封； (4) Cut a sample weighing 25-60 mg as a sample for differential scanning calorimetry analysis, press the tantalum cover with a tantalum sheet, insert the bottom of the tantalum cover into one end of a tantalum tube with a length of about 10-20 mm, and keep the tantalum cover The upper part is flush with the bottom edge of the tantalum tube, and then the tantalum cover and the tantalum tube are welded and sealed in the glove box;
(5)在手套箱内将切割好的样品放入钽管并将其密封，将密封有样品的钽管在手套箱外封入真空石英管中，然后将石英管放入热处理炉中退火，完成后将钽管取出，置入差示扫描量热分析仪支架进行差热分析。 (5) Put the cut sample into the tantalum tube in the glove box and seal it, seal the tantalum tube with the sample in the vacuum quartz tube outside the glove box, then put the quartz tube into the heat treatment furnace for annealing, complete Finally, the tantalum tube was taken out and placed in the support of a differential scanning calorimeter for differential thermal analysis.
优选地，所述的合金粉末为镁合金粉末或者铝合金粉末或者锌合金粉末或者锰合金粉末或者锶合金粉末或者钇合金粉末或者钕合金粉末，其中高挥发性、高反应活性元素镁、铝、锌、锰、锶、钇、钕的含量分别为99.0wt%～99.99wt% 。 Preferably, the alloy powder is magnesium alloy powder or aluminum alloy powder or zinc alloy powder or manganese alloy powder or strontium alloy powder or yttrium alloy powder or neodymium alloy powder, wherein the highly volatile and highly reactive elements magnesium, aluminum, The contents of zinc, manganese, strontium, yttrium and neodymium are respectively 99.0wt% to 99.99wt%.
作为改进，在合金样品的热分析过程中，保持样品水氧含量为0.4～1.0ppm。 As an improvement, during the thermal analysis of the alloy sample, the water and oxygen content of the sample is kept at 0.4-1.0 ppm.
本发明所要解决的关键技术是镁、铝、锌等合金所含高挥发性和高反应活性对样品制备和热分析带来的负面影响。针对镁、铝、锌等合金的高反应活性，必须构成一个低氧低水分的环境，来保证样品不与氧气和水反应。本发明采用手套箱来保证镁、铝、锌等合金从制备开始到热分析全过程保持较低的水氧含量。手套箱是将高纯惰性气体（氩气、氮气等）充入箱体内，并循环过滤掉其中的活性物质的实验设备。在手套箱中，首先将水和氧的含量降低到1ppm以下，随后开始合金样品的制备和检测。这样就保证了合金样品不会跟氧气和水反应。针对镁、铝、锌等合金的高挥发性，本发明设计了密封的钽坩埚。通过在手套箱中，将合金样品密封装入钽坩埚中，使得挥发的金属蒸汽停留在钽坩埚内部，进而保证试样的质量损失较小。制备一个合金样品只需要约0.4～0.6克金属原料，传统方法制备一个合金需要几百克甚至几千克金属原料。本发明解决了含高挥发性、高反应活性元素的样品难以制备和热分析的难题。所提供的方法可广泛用于镁（铝、锌等）合金、稀土（锰、锶、钇、钕等）合金等含高活性和高挥发性元素的合金的制备及其热分析。通过同标准纯金属物质的熔点对比表明采用本发明的热分析方法测定的相变温度精度可以达到± 1°C。 The key technology to be solved by the present invention is the negative impact of high volatility and high reactivity contained in magnesium, aluminum, zinc and other alloys on sample preparation and thermal analysis. In view of the high reactivity of magnesium, aluminum, zinc and other alloys, a low-oxygen and low-moisture environment must be formed to ensure that the sample does not react with oxygen and water. The present invention uses a glove box to ensure that the magnesium, aluminum, zinc and other alloys maintain a relatively low water and oxygen content in the whole process from preparation to thermal analysis. The glove box is an experimental equipment that fills the box with high-purity inert gas (argon, nitrogen, etc.), and circulates and filters out the active substances in it. In the glove box, first reduce the content of water and oxygen to below 1ppm, and then start the preparation and testing of alloy samples. This ensures that the alloy sample does not react with oxygen and water. Aiming at the high volatility of magnesium, aluminum, zinc and other alloys, the present invention designs a sealed tantalum crucible. By sealing the alloy sample into the tantalum crucible in the glove box, the volatilized metal vapor stays inside the tantalum crucible, thereby ensuring that the mass loss of the sample is small. Only about 0.4-0.6 grams of metal raw materials are needed to prepare an alloy sample, while the traditional method requires hundreds of grams or even several kilograms of metal raw materials. The invention solves the difficult problem of difficult preparation and thermal analysis of samples containing elements with high volatility and high reactivity. The provided method can be widely used in the preparation and thermal analysis of magnesium (aluminum, zinc, etc.) alloys, rare earth (manganese, strontium, yttrium, neodymium, etc.) alloys containing highly active and highly volatile elements. Show that the phase transition temperature precision that adopts thermal analysis method of the present invention to measure can reach ± 1 DEG C by comparing with the melting point of standard pure metal substance.
具体实施方式 Detailed ways
下面结合实施例对本发明作进一步说明。 Below in conjunction with embodiment the present invention will be further described.
实施例1： Example 1:
(1) 在手套箱中，采用镁颗粒(99.9 wt.%)、锌颗粒 (99.9 wt.%)、铝粉 (99.9 wt.%)、银颗粒(99.9 wt.%)，用电子天平分别称取50mg； (1) In the glove box, use magnesium particles (99.9 wt.%), zinc particles (99.9 wt.%), aluminum powder (99.9 wt.%), silver particles (99.9 wt.%), and weigh them with an electronic balance Take 50mg;
(2) 把称好的样品密封至钽管（外径6.8mm、壁厚0.4mm、长度15mm）中，将密封有样品的钽坩埚从手套箱取出，将底部打磨平整； (2) Seal the weighed sample into a tantalum tube (outer diameter 6.8mm, wall thickness 0.4mm, length 15mm), take out the tantalum crucible with the sample sealed from the glove box, and polish the bottom;
(3) 将密封好的钽坩埚置入差示扫描量热分析仪的支架进行热分析。 (3) Put the sealed tantalum crucible into the support of the differential scanning calorimeter for thermal analysis.
通过同标准纯金属物质的熔点对比表明采用本发明的热分析方法测定的相变温度精度可以达到± 1°C。 The comparison of the melting point with the standard pure metal substance shows that the accuracy of the phase transition temperature measured by the thermal analysis method of the present invention can reach ± 1°C.
实施例2: Example 2:
对于二元系Mg-Sr的样品制备和热分析，具体实施过程如下： For the sample preparation and thermal analysis of the binary system Mg-Sr, the specific implementation process is as follows:
（1）在手套箱中，采用镁粉 (99.5 wt.%), 锶块 (99.5 wt.%)，用电子天平称取重量约为500mg的3个试样，混合均匀后，采用小型电动压片机将其压制成直径5mm，高度为6mm的圆柱； (1) In the glove box, magnesium powder (99.5 wt.%) and strontium block (99.5 wt.%) were used to weigh 3 samples weighing about 500 mg with an electronic balance. The tablet machine presses it into a cylinder with a diameter of 5mm and a height of 6mm;
(2) 用氩弧电焊机将小圆柱封装入外径为7mm，壁厚0.3mm，长度为40mm的钽管中，并将钽管从手套箱中取出，将钽管在真空环境下封装入石英管中。随后将试样放入扩散炉中经过烧结及退火处理，然后将样品淬火并取出，放入手套箱中。接着将钽管锯开，并将样品从钽管中取出，从样品中切取一块重约50mg的样品，打磨平整作为热分析的试样； (2) Use an argon arc welding machine to package the small cylinder into a tantalum tube with an outer diameter of 7mm, a wall thickness of 0.3mm, and a length of 40mm, and take the tantalum tube out of the glove box, and package the tantalum tube in a vacuum environment. in a quartz tube. Then the sample was put into a diffusion furnace for sintering and annealing treatment, then the sample was quenched and taken out, and put into a glove box. Then saw the tantalum tube, and take the sample out of the tantalum tube, cut a sample weighing about 50 mg from the sample, and polish it flat as a sample for thermal analysis;
(3)采用模具，用厚度为0.3mm的钽箔压制出外径6mm，壁厚0.3mm，高度为3mm的钽盖，采用线切割机，将外径6.8mm，壁厚0.4mm的钽管切成长度为15mm的小钽管； (3) Using a mold, use a tantalum foil with a thickness of 0.3mm to press a tantalum cover with an outer diameter of 6mm, a wall thickness of 0.3mm, and a height of 3mm. Use a wire cutting machine to cut the tantalum tube with an outer diameter of 6.8mm and a wall thickness of 0.4mm. A small tantalum tube with a length of 15mm;
(4) 将切割好的样品放入长15mm一端密封的钽管中，并将另外一端密封。将密封有样品的钽管在手套箱外封入真空石英管中，然后将石英管放入热处理炉中退火，完成后将钽管取出，置入差示扫描量热分析仪支架进行差热分析。 (4) Put the cut sample into a 15mm-long tantalum tube with one end sealed, and seal the other end. The tantalum tube sealed with the sample was sealed in a vacuum quartz tube outside the glove box, and then the quartz tube was annealed in a heat treatment furnace. After completion, the tantalum tube was taken out and placed in the differential scanning calorimeter bracket for differential thermal analysis.
实施例3： Example 3:
对于Ca-Mg-Mn体系的样品制备和热分析，具体实施过程如下： For the sample preparation and thermal analysis of the Ca-Mg-Mn system, the specific implementation process is as follows:
(1) 在手套箱中，采用镁粉 (99.5 wt.%), 锰粉 (99.5 wt.%)，钙颗粒(99.5 wt.%)，用电子天平称取体积为0.3cm3的3个试样，混合均匀后，采用小型电动压片机将其压制成直径5mm，高度为6mm的圆柱； (1) In the glove box, magnesium powder (99.5 wt.%), manganese powder (99.5 wt.%), calcium particles (99.5 wt.%) were used to weigh three samples with a volume of 0.3 cm 3 with an electronic balance. After mixing evenly, use a small electric tablet press to press it into a cylinder with a diameter of 5mm and a height of 6mm;
(2) 用氩弧电焊机将小圆柱封装入外径为7mm，壁厚0.3mm，长度为40mm的钽管中；将钽管从手套箱中取出，并在真空环境下封装入石英管中。随后将试样放入扩散炉中经过烧结及退火处理，然后将样品淬火并取出，放入手套箱中；接着将钽管锯开，并将样品从钽管中取出，从样品中切取一小块重约30mg的小块，打磨平整作为热分析的试样； (2) Use an argon arc welding machine to package the small cylinder into a tantalum tube with an outer diameter of 7mm, a wall thickness of 0.3mm, and a length of 40mm; take the tantalum tube out of the glove box and package it into a quartz tube in a vacuum environment . Then put the sample into a diffusion furnace for sintering and annealing, then quench the sample, take it out, and put it in the glove box; then saw the tantalum tube, take the sample out of the tantalum tube, and cut a small sample from the sample A small piece weighing about 30 mg should be ground flat as a sample for thermal analysis;
(3)采用模具，用厚度为0.3mm的钽箔压制出外径6mm，壁厚0.3mm，高度为3mm的钽盖，采用线切割机，将外径6.8mm，壁厚0.4mm的钽管切成长度为15mm的小钽管； (3) Using a mold, use a tantalum foil with a thickness of 0.3mm to press a tantalum cover with an outer diameter of 6mm, a wall thickness of 0.3mm, and a height of 3mm. Use a wire cutting machine to cut the tantalum tube with an outer diameter of 6.8mm and a wall thickness of 0.4mm. A small tantalum tube with a length of 15mm;
(4) 将切割好的样品放入长15mm一端密封的钽管中，并将另外一端密封，将密封有样品的钽坩埚取出，将底部打磨平整； (4) Put the cut sample into a tantalum tube sealed at one end with a length of 15mm, and seal the other end, take out the tantalum crucible with the sample sealed, and polish the bottom;
(5) 将密封好的钽坩埚置入差示扫描量热分析仪支架进行热分析。 (5) Put the sealed tantalum crucible into the support of differential scanning calorimeter for thermal analysis.
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